CN103153263A - Denture adhesive compositions - Google Patents

Denture adhesive compositions Download PDF

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Publication number
CN103153263A
CN103153263A CN201180012624XA CN201180012624A CN103153263A CN 103153263 A CN103153263 A CN 103153263A CN 201180012624X A CN201180012624X A CN 201180012624XA CN 201180012624 A CN201180012624 A CN 201180012624A CN 103153263 A CN103153263 A CN 103153263A
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China
Prior art keywords
approximately
adhesive composition
denture adhesive
composition
cation
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Inventor
贾扬塔·拉贾亚
罗伯特·斯科特·莱昂纳多
拉斐尔·埃德蒙多·布拉斯
佛朗哥·席尔瓦·梅代罗斯
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Procter and Gamble Ltd
Procter and Gamble Co
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Procter and Gamble Ltd
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Application filed by Procter and Gamble Ltd filed Critical Procter and Gamble Ltd
Priority to CN201610862558.XA priority Critical patent/CN107411973A/en
Publication of CN103153263A publication Critical patent/CN103153263A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/30Compositions for temporarily or permanently fixing teeth or palates, e.g. primers for dental adhesives
    • A61K6/35Preparations for stabilising dentures in the mouth

Abstract

Denture adhesive compositions having good hold and improved taste containing a salt of a copolymer of alkyl vinyl ether-maleic acid or anhydride. Compositions containing from about 25% to about 45%, by weight of the composition, of a salt of a copolymer of alkyl vinyl ether-maleic acid or anhydride containing a cationic salt function containing: i) from about 60% to about 72% cations selected from calcium, strontium, magnesium, or combinations thereof; ii) from 0% to about 10% sodium cations; iii) less than 1% zinc cations; and iv) from about 25% to about 40% of a free acid component; and further containing from about 15% to about 25%, by weight of the composition of a carboxymethyl cellulose having a molecular weight of from about 200,000 to about 1,000,000 daltons; and a carrier.; Methods of improving the adhesion of dentures to the oral cavity by applying such compositions to dentures, the oral cavity, or both, and thereafter securing the denture to the ridge or palate of the oral cavity.

Description

Denture adhesive composition
Invention field
Compositions of the present invention relates to the Denture adhesive of the salt that comprises the AVE/MA polymer.
Background of invention
Common removable denture, dental lamina etc. are comprised of the artificial tooth that is embedded on suitable dens supporter or pedestal.Comprise that the denture stability agent of Denture adhesive is for the space of filling between artificial tooth and gingiva or tissue.Before in artificial tooth is positioned over the oral cavity, the denture stability agent is administered to artificial tooth-tooth plate surperficial, for reaching perfect applying, it should contact gingiva and mucous membrane tissue equably.Not only because of the adhesion characteristics of denture stability agent, and for providing cushion or packing ring between artificial tooth and gingiva or tissue, thereby artificial tooth is positioned in the oral cavity securely, and the agent of preparation denture stability.
Over the years, people have carried out the Denture adhesive composition that improvement is researched and developed in sizable effort.Synthetic and natural polymer and natural gum separately, combination and using with multiple binding agent and other combination of materials, to attempt some defective of minimizing.These defectives comprise inadequate retentivity and remove the in disorder and difficult of residual adhesive from oral cavity and artificial tooth.And food may be stuck between wearer's artificial tooth and oral cavity in addition, and may there be the mouthfeel unexpected for the wearer in some component.
Known alkyl vinyl ether-maleic acid and salt thereof are used for Denture adhesive composition in the art.This type of openly comprises: the United States Patent (USP) 3,003,988 of authorizing the people such as Germann of announcing on October 10th, 1961; Nineteen ninety the United States Patent (USP) 4,980,391 of authorizing the people such as Kumar announced of December 25 days; December in 1991 was announced on the 17th authorizes the people's such as Holeva United States Patent (USP) 5,073,604; The United States Patent (USP) 5,900,470 of authorizing the people such as Prosise of announcing on May 4th, 1999; The United States Patent (USP) 5,037,924 of authorizing the people such as Tazi of announcing on August 6th, 1991; The United States Patent (USP) 5,082,913 of authorizing the people such as Tazi of announcing on January 21st, 1992; With the United States Patent (USP) of authorizing Clarke 5,525,652 of everyday announcing June 11 in 1996.In addition, joint strip or embedded Denture adhesive are also known.Although have above-mentioned technique and a lot of other technique, still need to provide the denture stability compositions of the mouthfeel of good retentivity and improvement.
According to the present invention, by using Denture adhesive composition can obtain the mouthfeel feature of good retentivity and improvement, described compositions comprises alkyl vinyl ether-maleic acid, and described copolymer comprises the combination together with the specified quantitative free acid of magnesium, strontium and calcium salt.
Summary of the invention
The present invention relates to comprise the Denture adhesive composition of salt of the copolymer of alkyl vinyl ether-maleic acid or maleic anhydride, wherein said adhesive composition comprises: by weight of the composition approximately 25% to the about salt of the copolymer of alkyl vinyl ether-maleic acid of 45% or maleic anhydride, the salt of described copolymer comprises cationic salts functional group, and described cationic salts functional group comprises: approximately 60% to about 72% the cation that is selected from calcium, strontium, magnesium or their combination; 0% to about 10% sodium cation; Zinc cation less than 1%; With approximately 25% to about 40% free acid component; Wherein said compositions also comprise by weight of the composition approximately 15% to approximately 25% have approximately 200,000 to the about carboxymethyl cellulose of 1,000,000 daltonian molecular weight; And carrier.
The invention still further relates to the Denture adhesive composition of the salt of the copolymer that comprises alkyl vinyl ether-maleic acid or maleic anhydride, wherein said adhesive composition is comprised of following material basically: by weight of the composition approximately 25% to the about salt of the copolymer of alkyl vinyl ether-maleic acid of 45% or maleic anhydride, the salt of described copolymer comprises cationic salts functional group, and described cationic salts functional group is comprised of following material basically: i) approximately 60% to about 70% calcium cation; Ii) 0% to about 5% sodium cation; Iii) be substantially free of zinc cation; And iv) approximately 25% to about 35% free acid component; By weight of the composition approximately 15% to approximately 25% have approximately 500,000 to the about carboxymethyl cellulose of 900,000 molecular weight; And carrier, described carrier comprises water-insoluble liquid, gel, solid thermoplastics or their combination.
The invention still further relates to the such composition that cationic salts wherein functional group is substantially free of zinc cation.
The invention still further relates to cationic salts wherein functional group basically by calcium cation and about 25% above-mentioned composition that forms to about 35% free acid component.
The invention still further relates to wherein cationic salts functional group basically by approximately 65% to about 70% calcium cation, approximately 0% to about 5% sodium cation and about 28% above-mentioned composition that forms to about 32% free acid component.The invention still further relates to wherein said adhesive composition and comprise by weight of the composition approximately 15% to the about above-mentioned composition of 25% carboxymethyl cellulose.
The invention still further relates to wherein said carboxymethyl cellulose and have approximately 600,000 to the about above-mentioned composition of 800,000 molecular weight.
The salt that the invention still further relates to the copolymer of alkyl vinyl ether-maleic acid wherein or maleic anhydride has greater than 1,250, the above-mentioned composition of 000 molecular weight.
The invention still further relates to wherein when when measuring with 1% in methyl ethyl ketone solution under 25 ℃, the salt of the copolymer of alkyl vinyl ether-maleic acid or maleic anhydride has approximately 2.5 to the about above-mentioned composition of 3.8 specific viscosity.
The invention still further relates to the above-mentioned composition that also comprises one or more compositions, described composition choosing is the group of following composition freely: additional adhesive component, plasticizer, coloring agent, antiseptic, thickening agent, carrier, flavoring agent, aromatic, sensory agent and their mixture.
The invention still further relates to wherein said cationic salts functional group basically by approximately 65% to about 70% calcium cation and about 28% above-mentioned composition that forms to about 32% free acid component.
The invention still further relates to wherein said adhesive composition comprise by weight of the composition approximately 15% to approximately 25% have approximately 600,000 to the about above-mentioned composition of the carboxymethyl cellulose of 800,000 molecular weight.
The salt that the invention still further relates to the copolymer of alkyl vinyl ether-maleic acid wherein or maleic anhydride has greater than 1,250, the above-mentioned composition of 000 molecular weight.
The invention still further relates to wherein when when measuring with 1% in methyl ethyl ketone solution under 25 ℃, the salt of the copolymer of alkyl vinyl ether-maleic acid or maleic anhydride has approximately 2.5 to the about above-mentioned composition of 3.8 specific viscosity.
The invention still further relates to the above-mentioned composition that also comprises at least one non-binding agent self-supporting layer.
The invention still further relates to the above-mentioned composition that carrier wherein comprises microwax.
The invention still further relates to the above-mentioned composition that wherein said compositions is substantially free of magnesium.
The invention still further relates to the above-mentioned composition that wherein said compositions is substantially free of sodium.
The invention still further relates to the above-mentioned composition that wherein said compositions is substantially free of strontium.
The invention still further relates to a kind of artificial tooth that improves to the adhering method in oral cavity, wherein any above-mentioned composition is administered to artificial tooth, oral cavity or both and the ridge or the palate that afterwards artificial tooth are fixed to the oral cavity.
Detailed Description Of The Invention
Denture adhesive composition of the present invention comprises the carboxymethyl cellulose with the magnesium of alkyl vinyl ether-maleic acid, strontium and/or calcium salt combination, the salt of described copolymer has specific free acid content, randomly comprises 0% to about 10% sodium cation; And be substantially free of zinc cation.
Described adhesive composition can be goods, powder, cream, paste, liquid, aerosol and/or wafer form.Powder type can be sprinkling upon on artificial tooth, and then moistening embeds in the oral cavity.Described compositions also can be sent excipient composition with multiple routine, can be applied to artificial tooth and to embed liquid or paste in the oral cavity to form.These compositionss optionally comprise at least one non-binding agent self-supporting layer.Denture adhesive composition with self-supporting layer can and be administered to artificial tooth by abundant moistening.The below provides the detailed description of solvent of the present invention and optional components.
Definition
As used herein, term " safe and effective amount of binder " refers to be enough to provide to the oral cavity adhesiveness and/or the adhesion of artificial tooth to oral cavity palate and dental ridge is provided, and to the user avirulence, to the oral cavity tissue not damaged, and does not change the amount of artificial tooth material.
As used herein, term " AVE/MA " refers to alkyl vinyl ether-maleic acid.As used herein, term " mixed polymer salt " or " salt-mixture " refer to the salt of AVE/MA, wherein have at least 2 kinds of different cationes to be mixed with each other on identical polymer or mix with other ester functional group.
As used herein, term " free acid " " (" FA ") component refer to AVE/MA unreacted carboxyl (COOH).
The percentage ratio that this paper be used for to describe copolymer salt functional group is defined in the stoichiometry percentage ratio of all initial carboxyls that react on polymer.Except as otherwise noted, all other percentage ratios used herein all by weight.
Polymer
Alkyl vinyl ether-maleic acid (" AVE/MA ") copolymer comprises constitutional repeating unit:
(I)
Figure GDA00003036040400051
Wherein R represents alkyl, is C in certain embodiments 1-C 5Alkyl, and n is the integer greater than, the representative number of times that construction unit repeats in polymer molecule.
Denture adhesive composition of the present invention comprises salt or the salt-mixture of AVE/MA copolymer, and wherein said salt comprises cationic salts functional group.Described cationic salts functional group comprises (or basically by forming, or by forming) approximately 60% to approximately 72% magnesium, strontium and/or calcium cation, and 0% to about 10% sodium cation; Less than 1% (or being substantially free of) zinc cation; With approximately 25% to about 40% free acid component.
The AVE/MA copolymer has the specific viscosity of certain limit.For example, when under 25 ℃ in methyl ethyl ketone solution during with the initial anhydride of the copolymer of 1% weight/volume or acidity test, described specific viscosity can be at least 2.0, or 2.5 or higher, or approximately 2.5 to approximately 5.In one embodiment, when when measuring with 1% in methyl ethyl ketone solution under 25 ℃, the salt of the copolymer of alkyl vinyl ether-maleic acid or maleic anhydride has approximately 2.5 to about 3.8 specific viscosity.
Described AVE/MA copolymer has at least about 1,250,000 daltonian molecular weight.In some embodiments, described molecular weight is approximately 1,500,000 to approximately 3,000,000, or approximately 1,700,000 to approximately 2,100,000, or approximately 1,800,000 to about 2,000,000 dalton.
Commercially available acquisition and the AVE/MA copolymer that is used for this paper comprise GANTREZ AN169 or the GANTREZ179 available from International Specialty Products, and according to their brief introduction material, it has respectively approximately 1,980,000 and 2,400,000 typical molecular weight.The polymer of the commercially available acquisition that another kind is suitable is for deriving from equally the AN169BF of International Specialty Products.
The AVE/MA copolymer reaction forms the salt that comprises cationic salts functional group.Described cationic salts functional group comprises approximately 60% to about 72% cation, and described cation is selected from calcium, strontium, magnesium and their combinations.In some embodiments, described cationic salts functional group comprises approximately 60% to approximately 70%, or approximately 61% to approximately 69%, or approximately 62% to approximately 68%, or approximately 63% to about 67% cation, described cation is selected from calcium, strontium, magnesium and their combinations.In some embodiments, the content of magnesium cation in described cationic salts functional group can be any combination of following scope: approximately 1%, 5%, 10%, 15% of primary response carboxyl, 20%, 25%, 30%, 35%, or 40% to approximately 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69% or 70%.In some embodiments, the content of strontium cation in described cationic salts functional group can be any combination of following scope: approximately 1%, 5%, 10%, 15% of primary response carboxyl, 20%, 25%, 30%, 35%, or 40% to approximately 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69% or 70%.In some embodiments, the content of calcium cation in described cationic salts functional group can be any combination of following scope: approximately 1%, 5%, 10%, 15% of primary response carboxyl, 20%, 25%, 30%, 35%, or 40% to approximately 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69% or 70%.
In some embodiments, described cationic salts functional group can comprise 0% to approximately 10%, or 0% to approximately 5%, or approximately 1% to approximately 4%; Approximately 1% to approximately 3%, or approximately 0.5% to about 2% sodium cation.In some embodiments, described cationic salts functional group can be substantially free of ferrum, manganese, zinc, copper, sodium, potassium, zirconium, strontium, magnesium and/or aluminum.In some embodiments, described cationic salts functional group is substantially free of zinc cation.Without being limited by theory, by the cationic amount of zinc (with other metal) in restriction cationic salts functional group, can improve the whole mouthfeel of described product.Known zinc has the mouthfeel (referring to for example United States Patent (USP) 6,169,118) of making us unhappy, therefore can expect to prepare the compositions that does not substantially contain generally zinc.Phrase " is substantially free of " and refers to less than 0.0001%, preferably less than 0.001%, is more preferably less than 0.01%, and is more preferably less than 0.1%.
In some embodiments, described cationic salts functional group comprises approximately 25% to about 40% free acid component.In other embodiments, described free acid component can be any combination of following scope: approximately 25%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, or 39% to approximately 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, or 40%.Without being limited by theory, the amount of free acid component is important, because relatively large free acid can provide more site, to provide adhesion to wet mucous membrane surface.In addition, it is believed that a certain amount of free acid also can be used for optimizing the interaction with coadhesive such as carboxymethyl cellulose.Yet too much free acid may reduce metal corsslinking, and/or increases the dissolubility of polymer salt, therefore reduces cohesive.Therefore, the amount of free acid component is important for the good adhesion that realizes the present composition (compositions that especially comprises coadhesive such as carboxymethyl cellulose).
Copolymerization by making alkyl vinyl ether monomer (as methyl vinyl ether, ethyl vinyl ether, divinyl ether, propyl vinyl ether and IVE) and maleic anhydride obtains the alkyl vinyl ether copolymer-maleic anhydride to generate the alkyl vinyl ether-copolymer-maleic anhydride that is easy to accordingly be hydrolyzed into acid copolymer.Method such as US2 that suitable copolymer can be known by prior art, 782,182 and US2,047,398 makes.Anhydride and sour form are also all available from commercial supplier.For example, GAF Corporation (Wayne, N.J.) provides polymerization free acid form (I) and corresponding anhydride form with " GANTREZ S series " under its " GANTREZ " trade mark and " GANTREZ AN series " respectively.When acid anhydride copolymer was soluble in water, the anhydride bond fracture was with the polymerization free acid (I) of height of formation polarity.Therefore, can use and compare comparatively cheap anhydride form with sour form as the convenient and more cheap precursor of acid.Can advantageously adopt high temperature to improve anhydride-extremely-acid-hydrolyzed speed.
Can interact by the compound (as hydroxide, oxide, acetas, halogenide, lactate etc.) that makes AVE/M anhydride or the acid copolymer with at least a cationic salts functional group (as magnesium, strontium or calcium and optional sodium) and have a functional group that is typically the carboxylic acid reaction thing in water-bearing media, can make the salt form of this motif polymerization thing.In one embodiment, utilize magnesium oxide, Strontium hydrate., strontium carbonate and/or calcium hydroxide.
Should avoid forming the ion of toxicity, zest or pollutant byproducts, or extraordinary precaution and processing are provided, to guarantee eliminating and do not exist this type of by-product in the polymer salt end-product.Particular compound used should be basically pure, to guarantee to obtain basically pure polymer salt end-product.
The aqueous dispersion of granulated metal compound can mix with the serosity form with powder polymer, presents in an amount at least sufficient to provide suitable cations desired in end-product.This completes at ambient temperature, then slowly is heated to 70-95 ℃, and simultaneously continuous vigorous stirring is to prevent the localized precipitation of cationic polymer salt; Continue to stir with guarantee all salt-forming compounds all with described copolymer reaction.
Alternatively, described polymer can be in the aqueous mixture or serosity of one or more bivalence and/or monovalence metal base, by with polymer/alkali mixture heated to about 45 ℃ of temperature to about 100 ℃ of scopes, be hydrolyzed and neutralize.In above-mentioned any method, gained serosity or solution can be transferred in the dry tray of rustless steel, and place a period of time (approximately 18-24 hour) that is enough to evaporation reaction medium (water) and removes water from polymer in the forced ventilation machinery convection oven of 60-70 ℃.Alternatively, gained serosity or solution can reclaim described polymer with the vapours tumble drying with evaporation water content and with sheet form under 100 ℃ to 200 ℃.After drying, polymer formation is easy to the fragility thin slice peeled off from tray or drum surface, and grinds to form as required fine powder, so that gratifying denture stability characteristic to be provided.The method for preparing the salt of these AVE/MA polymer is disclosed in further that December in 1991 announced on the 17th authorizes the people's such as Holeva United States Patent (USP) 5,073,604, and announced on February 16th, 1999 authorize the people's such as Liang 5,872,161; Announced on November 3rd, 1998 authorize the people such as Synodis 5,830,933 in.
Described salt polymer has good mouthfeel and/or adheres to quality when contacting with water or saliva, make them especially can be used as denture adhesive agent material in the artificial tooth compositions.Compositions of the present invention comprises the salt polymer of safe and effective bonding amount, be in some embodiments at least 10 % by weight, 20 % by weight, 30 % by weight or 40 % by weight, described salt polymer is unique adhesive component or common binding agent for being combined with other adhesive component.
Carboxymethyl cellulose
The Denture adhesive composition of this paper also comprises by the weighing scale of described adhesive composition approximately 10% to approximately 30%, and is optional approximately 15% to approximately 25%, or approximately 17% to about 20% carboxymethyl cellulose.In one embodiment, described carboxymethyl cellulose is sodium carboxymethyl cellulose.The carboxymethylcellulomaterials materials that is used for this paper comprises those with at least 200,000 daltonian molecular weight.In some embodiments, carboxymethyl cellulose has approximately 200,000 to approximately 1,000,000, or approximately 500,000 to 900,000, or approximately 600,000 to about 800,000 daltonian molecular weight.The example of carboxymethyl cellulose that is used for the commercially available acquisition of this paper comprises the 7H series carboxymethyl cellulose available from Aqualon, and according to their brief introduction material, it has approximately 700,000 daltonian typical molecular weight.Other example of the carboxymethyl cellulose of commercially available acquisition comprises the 7H3SX8F that derives from Aqualon/Hercules, and derives from the CEKOL30 of C.P.Kelco/Noviant/Huber, 000P.
Carrier
Denture adhesive composition of the present invention comprises approximately 2% to approximately 80%, and in another embodiment approximately 30% to about 70% carrier, as water-insoluble liquid, gel, solid thermoplastics or their combination.
In general, can use the water-insoluble blend of mineral oil and vaseline to make described compositions become suspension.This suspension of solid particle in the liquid/gel excipients/carriers also is called as Denture adhesive cream or paste.In some embodiments, compositions of the present invention comprises the water-msoluble ingredients (wic) of safe and effective amount.In one embodiment, the content of this component can be by weight of the composition approximately 2%, 5%, 10%, 20%, 25%, 30%, 35% to approximately 45%, 50%, 60%, 70%, 90% or their any combination.In other embodiments, the content of described water-msoluble ingredients is by weight of the composition approximately 20% to approximately 70%, approximately 25% to approximately 60%, or approximately 35% to approximately 60%.In another embodiment, described water-msoluble ingredients in water for basically non-swelling.In some embodiments, the swellbility of described non-swelling water-msoluble ingredients in water is less than approximately 10%, 5%, 2% or 1%.
In one embodiment, described water-msoluble ingredients comprises liquid, gel or their mixture.In one embodiment, the group of the free following composition of described water-msoluble ingredients choosing: native paraffin, synthetic wax, vaseline, polyvinyl acetate, natural oil, artificial oil, fat, siloxanes, silicone derivative, polydimethylsiloxane, organic siliconresin, hydrocarbon, hydrocarbon derivative, quintessence oil, caprylic/capric triglyceride, polybutene, oleic acid, stearic acid and their combination.In another embodiment, described water-msoluble ingredients comprises vaseline, polyvinyl acetate, natural oil, artificial oil, fat, siloxanes, silicone derivative, polydimethylsiloxane, organic siliconresin, hydrocarbon, hydrocarbon derivative, polybutene, oleic acid, stearic acid, quintessence oil or their combination.
The example of natural oil includes but not limited to vegetable oil (deriving from Semen Maydis oil), soybean oil, Oleum Gossypii semen, Petiolus Trachycarpi oil, Oleum Cocois, mineral oil, animal oil (deriving from fish oil) etc.The example of artificial oil includes but not limited to silicone oil etc.In one embodiment, described water-msoluble ingredients comprises natural oil.In another embodiment, described water-msoluble ingredients is substantially free of vaseline.In another embodiment, described water-msoluble ingredients also comprises vaseline.In other embodiments, described water-msoluble ingredients can comprise vaseline, for example derives from the vaseline numbering 4,5,10,15 or 20 of Calumet Specialty product.
In another embodiment, described natural oil comprises mineral oil.In one embodiment, the content of mineral oil in described compositions is approximately 30% to approximately 50%, and is approximately 35% to approximately 45% in another embodiment.In some embodiments, described mineral oil can be slab oil, light mineral oil or industrial mineral oil.Light mineral oil can be for example Drakeol5,10,13 or 15.Slab oil can be for example Drakeol19,21,34,35 or 600.
In some embodiments, water-msoluble ingredients comprises wax.Wax generally is made of many kinds of substance, comprises hydrocarbon (normal chain or branched paraffin and alkene), ketone, diketone, primary alconol and secondary alcohol, aldehyde, sterol ester, alkanoic acid, terpenes (Squalene) and monoesters (wax ester).dissimilar wax comprises animal wax and insect wax (Cera Flava, Chinese wax, shellac wax, spermaceti, lanoline), vegetable wax (bayberry wax, candelilla wax, Brazil wax, castor wax, esparto wax, Japan wax, Jojoba oil, ouricury wax, rice bran wax), mineral wax (cresin wax, montanin wax, ceresine, peat wax), pertroleum wax (paraffin or microwax), and synthetic wax (Tissuemat E, Fischer-Tropsch wax, chemical modification wax, substituted amide wax, the alpha-olefin of polymerization).
In one embodiment, described water-msoluble ingredients comprises natural or synthetic wax.In another embodiment, the group of the free following composition of described native paraffin choosing: animal wax, vegetable wax, mineral wax and their combination.In another embodiment, described animal wax comprises Cera Flava, lanoline, shellac wax, Chinese wax and their combination.In another embodiment, described vegetable wax comprises Brazil wax, candelilla wax, bayberry, Caulis Sacchari sinensis and their combination; And mineral wax comprises mineral tallow or ceresine (ceresine, ceresin, montan wax) and pertroleum wax such as paraffin and microwax and their combination.In one embodiment, the wax of this paper is the native paraffin of the group of the free following composition of choosing: Cera Flava, candelilla wax, candle wax, Brazil wax, paraffin and their combination.In different embodiments, the content of wax can be approximately 1%, 2%, 5%, 8% to approximately 5%, 10%, 20%, 30%, or their any combination.
In another embodiment, native paraffin comprises paraffin.The paraffin that is used for this paper can have approximately 65 ℃ to approximately 80 ℃, and about 70 ℃ of extremely about melting ranges of 75 ℃ in another embodiment.In another embodiment, the microwax that is used for this paper can have approximately 65 ℃ to approximately 90 ℃, and about 80 ℃ of extremely about fusing points of 90 ℃ in another embodiment.In one embodiment, the Cera Flava that is used for this paper can have approximately 62 ℃ to the approximately fusing point of 65 ℃ and the flash-point of 242 ℃.In another embodiment, the candelilla wax that is used for this paper can have approximately 68 ℃ to the about fusing point of 72 ℃.In additional embodiment, the Brazil wax that is used for this paper can have approximately 83 ℃ to the about fusing point of 86 ℃.In one embodiment, the Fischer-Tropsch wax that is used for this paper can have approximately 95 ℃ to the about fusing point of 120 ℃.Also can obtain to have Cera Flava, candelilla wax, Brazil wax with the artificial grade of the Cera Flava similarity of natural grade.
In one embodiment, water-msoluble ingredients comprises vaseline." Condensed Chemical Dictionary " the 13rd edition (John Wiley﹠amp according to Hawley; Sons, 1997), vaseline is " mixture of the hydrocarbon that obtains by distillation paraffin-base petroleum fraction "; And according to " the The United States Pharmacopia " of 2005, vaseline was " available from the purified mixture of the semi-solid hydrocarbon of oil ".It also is called as " natural vaseline ".According to 2005 " The United States Pharmacopia; vaseline it is said to have fusion range between 38 ℃ and 60 ℃; and according to " the The Merck Index " the 10th edition of nineteen eighty-three, vaseline it is said to have fusion range between 38-54 ℃.Vaseline can be multiple grade obtain, according to Sonneborn Inc product manual, adopt ASTM D-937 to record, it has 180 " cone penetration values " to about 245 scopes.
In one embodiment, described water-msoluble ingredients has greater than the about fusing point of 60 ℃.In some embodiments, described water-insoluble thermoplastic component has approximately 35 ℃, and 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, to approximately 110 ℃, 120 ℃, 150 ℃, 175 ℃, the fusing point of 200 ℃ and/or their any combination are with formation scope, starting point and/or terminal point.In another embodiment, described compositions is substantially free of and has higher than the about water-insoluble thermoplastic component of 75 ℃ of fusing points.
In some embodiments, described carrier comprises microwax.Microwax can be refine and/or basically pure.In additional embodiment, vaseline does not provide microwax." Encyclopedia of Polymer Science and Engineering " the 2nd edition, the 17th volume, the 788th page of molecular weight ranges of describing microwax is 450 to 800, thus described document incorporated into way of reference." Kirk-Othmer Encyclopedia of Chemical Technology " the 5th edition, the 26th volume is described microwax for the 216th page and is had following typical characteristics: flash-point, closed-cup, 260 ℃; Viscosity under 98.9 ℃, 10.2-25mm 2/ s; Fusion range, 60 ℃-93 ℃; Refractive index under 98.9 ℃, 1.435-1.445; Mean molecule quantity, 600-800; Carbon atom in per molecule, 30-75; And the ductility/degree of crystallinity of solid wax is prolonged and is moulded to tough crisp, and in one embodiment, viscosity index improver has these concrete characteristics, thus described document is incorporated herein by reference.
In another embodiment, described microwax have scope be approximately 50 ℃ to the about fusing point of 100 ℃.In other embodiments, it is approximately 50 ℃ that microwax has scope, 55 ℃, and 60 ℃, 65 ℃, 70 ℃ to approximately 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, the fusing point of any combination of 100 ℃ or they.In a particular, described microwax have scope be approximately 75 ℃ to the about fusing point of 85 ℃.
In another embodiment, described microwax is made by Crompton, Sonneborn (Witco), and is called
Figure GDA00003036040400111
And with trade mark
Figure GDA00003036040400112
Sell.This wax have scope be approximately 73.9 ℃ to the about fusing point of 79.4 ℃ (adopting ASTM D-127 to record), have under 25 ℃ approximately 60 to about 80 osmotic value (adopting ASTM D-1321 to record), have under 98.9 ℃ approximately 75 to the about kinematic viscosity of 90 Saybolt universal seconds (adopting ASTM D-2161 to record), have COC at least about 246 ℃ (cup is opened in the Cleveland) flash-point (adopting ASTM D-92 to record), and have approximately 68 ℃ to the about freezing point of 77 ℃ (adopting ASTM D-938 to record).
In another embodiment, described microwax is made by Crompton, Sonneborn (Witco), and is called
Figure GDA00003036040400121
And with trade mark
Figure GDA00003036040400122
Sell.This wax have scope be approximately 79 ℃ to the about fusing point of 87 ℃ (adopting ASTM D-127 to record), have under 25 ℃ approximately 15 to about 22 osmotic value (adopting ASTM D-1321 to record), has under 98.9 ℃ the kinematic viscosity (adopting ASTM D-2161 to record) at least about 75 Saybolt universal seconds, have COC at least about 277 ℃ (cup is opened in the Cleveland) flash-point (adopting ASTM D-92 to record), and have approximately 75 ℃ to the about freezing point of 82 ℃ (adopting ASTM D-938 to record).
In another embodiment, described microwax is made by Crompton, Sonneborn (Witco), and is called
Figure GDA00003036040400123
And with trade mark Sell.This wax have scope be approximately 77 ℃ to the about fusing point of 82 ℃ (adopting ASTM D-127 to record), have under 25 ℃ approximately 25 to about 35 osmotic value (adopting ASTM D-1321 to record), have under 98.9 ℃ approximately 75 to the about kinematic viscosity of 90 Saybolt universal seconds (adopting ASTM D-2161 to record), have COC at least about 277 ℃ (cup is opened in the Cleveland) flash-point (adopting ASTM D-92 to record), and have approximately 72 ℃ to the about freezing point of 77 ℃ (adopting ASTM D-938 to record).
Although microwax and paraffin are pertroleum wax, still there is concrete difference between them.Microwax is the refining mixture of the solid-state saturated aliphatic hydrocarbon of the preparation of deoiling from some fraction in PETROLEUM PROCESSING technique.With the more familiar paraffin phase ratio that mainly comprises unbranched alkane, microwax comprises isoparaffin (branched-chain hydrocarbons) and the cycloalkane of higher percent.It is characterized in that the fineness with its crystal of comparing than megacryst of paraffin.Its saturated aliphatic hydrocarbon by high molecular forms.Its generally than paraffin more black, more viscous, denseer thick, have more viscosity and have more elasticity, and have higher molecular weight and fusing point.The elasticity of microwax and viscous characteristics are relevant to the non-straight chain component that they comprise.General microwax crystal structure is little and thin, makes them have more than paraffin flexible.
According to " Encyclopedia of Polymer Science and Engineering " the 17th volume in 1989, the 788th page of (John Wiley﹠amp; Sons): the molecular weight ranges of paraffin is about 280 to 560 (C20-C40); The molecular weight ranges of microwax is 450-800 (C35-C60).The amount of the normal alkane in paraffin surpasses 75% usually, and can be up to 100%; Microwax mainly is comprised of saturated isoalkane and saturated rings alkane and some normal alkane.
" Kirk-Othmer Encyclopedia of Chemical Technology " (John Wiley﹠amp according to 2005; Sons): paraffin has number-average molecular weight and the per molecule 20-36 carbon of 350-420; And microwax has number-average molecular weight and the per molecule 30-75 carbon of 600-800.Paraffin is coarse-grain, fragility, and formed with remaining C18-C36 isoalkane and cycloalkane by the normal alkane of 40-90%.Paraffin is the pertroleum wax that mainly is comprised of normal alkane.Microwax is for also comprising the side chain of remarkable ratio and the pertroleum wax of cyclic saturated hydrocarbon except normal alkane.Developed based on the refractive index of wax and the taxonomic hierarchies of freezing point (being measured by ASTM D-938) thereof.Paraffin has the refractive index at 98.9 ℃ of lower 1.430-1.433; And microwax has the refractive index at 98.9 ℃ of lower 1.435-1.445.Paraffin is frangible to crystallization; Microwax is to prolong to mould to tough crisp.Paraffin has affinity hardly to oil; Microwax has strong affinity to oil.Different from paraffin, oil is firmly remained in the lattice of microwax, and can not migrate to the surface." Condensed Chemical Dictionary " the 13rd edition (John Wiley﹠amp according to Hawley; Sons, 1997), paraffin it is said to have the approximately fusing point of 47-65 ℃, and according to " Kirk-Othmer Encyclopedia of Chemical Technology " (John Woley﹠amp; Sons, 2005), paraffin it is said the fusing point with 46-68 ℃." Condensed Chemical Dictionary " the 13rd edition (John Wiley﹠amp according to Hawley; Sons), microwax has the approximately fusing point of 63-88 ℃, and according to " Kirk-Othmer Encyclopedia of Chemical Technology " (John Woley﹠amp; Sons, 2005), microwax has the fusing point of 60-93 ℃.
In some embodiments, be used for the present invention's water-insoluble thermoplastic component and/or viscosity index improver and have approximately 5,10,15,20,25,30,35,40,45,50,55,60 to approximately 25,30,35,40,45,50,55,60,65,70,75,80,85,90,95,100,110,120,250 osmotic value, with any combining form of numeral with the formation scope.
In some embodiments, described water-insoluble thermoplastic component and/or viscosity index improver such as microwax have the mean molecule quantity higher than vaseline.In some embodiments, compare with the blend of vaseline combination with mineral oil, the MW of described water-msoluble ingredients and/or viscosity index improver is higher, and branching, more pliable and tougher more, and is more firm, more tough and tensile, and fusing point is higher, and/or degree of crystallinity is larger.
Optional non-binding agent self-supporting layer
Denture adhesive composition of the present invention randomly comprises at least one non-binding agent self-supporting layer.Described non-binding agent self-supporting layer is characterised in that it can keep the intensity of adhesive composition and adhesive composition is provided under the existence of water and/or saliva integrity.Described non-binding agent self-supporting layer can comprise material such as polyester, polypropylene, nylon, artificial silk, cellulose acetate, non-sticky cellulose derivative, cloth, fiber is grabbed floss, paper wood, plastics, leather, microwax, synthetic fibers, natural fiber and their mixture.Some embodiments can comprise non-sticky cellulose derivative, polyester, polypropylene, nylon, artificial silk, cloth, paper wood, microwax or their mixture.Some embodiments can comprise polyester, polypropylene, artificial silk, nylon, cloth and/or paper wood.
Described non-binding agent self-supporting layer can be any physical form that is suitable for providing to adhesive composition of the present invention intensity and/or integrity.This type of physical form comprises non-woven, woven, continuous, chopped and their combination.In addition, described non-binding agent self-supporting layer can be formed by the common known any method in this area.These class methods comprise non-Method for bonding, the sticking method of spray, spun-bond process, needle point method, carding method, hot sticky Heshui acupuncture manipulation, meltblown, hole printing Method for bonding, pin stitch, wet-laying method, dry-laying method and their combination.
Other adhesive component
Compositions of the present invention also can comprise other adhesive component.If present, these adhesive components use with safe and effective bonding amount.In general, the content of other adhesive component can be by weight of the composition approximately 0%, 10%, 20%, 30%, or 40% to approximately 50%, 60%, 70%, 80%, or any combination in 90% scope.
Suitable adhesive component comprises having water solublity hydrophilic colloid or the polymer that swelling when being exposed to moisture forms the characteristic of gluing agglomerate.This type of adhesive material comprises natural gum, synthetic polymer natural gum, the acid of AVE/MA copolymer, AVE/MA copolymer anhydride, AVE/MA/IB, synthetic polymer, mucoadhesive polymer, hydrophilic polymer, sugar derivatives, other cellulose derivative and the adhesive material that is usually used in the denture stability compositions and holds with motif polymerization phase of the present invention and their mixture.The example of materials comprises karaya, guar gum, gelatin, Algin, sodium alginate, Tragacanth, chitosan, Polyethylene Glycol, acrylamide polymer, acrylate copolymer, polyvinyl alcohol, polyamine, polyquaternary ammonium salt compound, polybutene, siloxanes, ethylene oxide polymer, polyvinylpyrrolidone, cationic polyacrylamide polymer.
In some embodiments, materials can be other cellulose derivative, Polyethylene Glycol, poly(ethylene oxide), karaya, sodium alginate, chitosan, polyvinyl alcohol or their mixture.In other embodiments, described material can be other cellulose derivative, as methylcellulose, hydroxyethyl-cellulose, hydroxypropyl cellulose, hydroxypropyl emthylcellulose or their mixture.
Other composition
The Denture adhesive composition of the present invention that also comprises non-binding agent self-supporting layer also can comprise coating, and described coating is adhered to dry artificial tooth, and if exist, will be placed on the one side of Denture adhesive composition.The applicable compositions of making the type adhesive phase comprises polybutene, siloxanes, rubber, vaseline, natural polymer, synthetic polymer and their mixture.The content of described adhesive phase can be by weight of the composition approximately 0% to approximately 70%, is approximately 0.5% to approximately 20% in some embodiments.
Other suitable composition can comprise coloring agent, antiseptic such as methyl parahydroxybenzoate and propyl p-hydroxybenzoate; Thickening agent such as silicon dioxide and Polyethylene Glycol; And excipient such as Albolene, vaseline, mineral oil and glycerol.In some embodiments, can comprise Polyethylene Glycol, silicon dioxide and/or vaseline.The content of coloring agent, antiseptic, thickening agent and excipient can be by weight of the composition approximately 0% to approximately 20%.
Compositions of the present invention also can comprise one or more components, and these components provide local flavor, fragrance and/or realizable beneficial effect (heating agent or coolant).Suitable component comprise natural or artificial sweeting agent, menthol, menthyl lactate, wintergreen oil, Oleum menthae, Oleum Menthae Rotundifoliae, folic alcohol, clove bud oil, anethole, methyl salicylate, cineole, Cortex cinnamomi japonici (Ramulus Cinnamomi), 1-menthyl acetate, Salvia japonica Thunb., acetaminol, parsley oil,
Figure GDA00003036040400151
Alkane ketone, α-ionone, Origanum majorana L., Fructus Citri Limoniae, orange, methylol anethole, Cortex Cinnamomi, vanillin, thymol, linalool, the cinnamic aldehyde glycerine acetal that is called as CGA and their mixture and coolant.
Coolant can be any various material.These materials comprise carboxylic acid amides, menthol, ketal, glycol and their mixture.In some embodiments, coolant in the present composition can be terpane carbamyl reagent, as the WS-3 of commodity " WS-3 " by name, the WS-23 of commodity " WS-23 " by name and their mixture.The group of the following composition of the optional freedom of additional coolant: menthol, the 3-1-menthoxypropane-1 that is called as TK-10 of being produced by Takasago, 2-glycol, the menthone glycerol ketals that is called as MGA of being produced by Haarmann and Reimer and the menthyl lactate that is called as Frescolat of being produced by Haarmann and Reimer.Term menthol used herein and menthyl comprise dextrorotation and laevoisomer and their racemic mixture of these compounds.TK-10 is described in 7/10/84 United States Patent (USP) 4,459,425 of authorizing the people such as Amano of announcing.WS-3 and other reagent are described in the United States Patent (USP) 4,136,163 of authorizing the people such as Watson of announcing on January 23rd, 1979.The content of these reagent can be by weight of the composition approximately 0% to approximately 50%.
Compositions of the present invention can be used as Denture adhesive and/or as the biological adhesive in wet tissue, described wet tissue such as mucosal tissue, wound, oral mucosa etc.Adhesive composition of the present invention can be used for sending to mucosa or wet tissue the therapeutic active substance that one or more are suitable for using topical.As used herein, the reagent that has pharmaceutically active when seeing through health wet tissue or mucous membrane surface such as oral cavity, wound absorbs or being administered on skin surface described in phrase " therapeutic active substance ".The content of therapeutic active substance can be by weight of the composition approximately 0% to approximately 70%.
The therapeutic active substance that is used for the present composition can comprise antimicrobial such as iodine, sulfonamide, two biguanide or phenolic resins; Antibiotic such as tetracycline, neomycin, kanamycin, metronidazole or clindamycin; Antiinflammatory such as aspirin, acetaminophen, naproxen and salt thereof, ibuprofen, ketorolac, flurbiprofen, indomethacin, acetaminol or hydrocortisone; Dentin desensitizer such as potassium nitrate, strontium chloride or sodium fluoride; Anesthetis such as lignocaine or benzocaine; Antifungal; Fragrance compound such as Camphora, Eucalyptus oil; Flavoring agent, aromatic or sensory agent (heat agent or coolant) and aldehyde derivatives such as benzaldehyde; Insulin; Steroidal compounds; And antineoplastic agent.Generally acknowledge in some form of therapy, for obtaining optimum efficiency, it may be effective using the combination of these reagent in identical delivery system.Therefore, for example, antimicrobial and antiinflammatory can be mixed in single delivery system so that the effect of combination to be provided.
Method for the preparation of compositions
Method for the preparation of Denture adhesive composition of the present invention (goods, cream, powder, wafer, liquid, aerosol, paste) comprises the disclosed conventional method in this area.Conventional method is set forth in the US5 that authorizes the people such as Clarke that announced on June 11st, 1996,525,652; The US3 that authorizes the people such as Germann that announced on October 10th, 1961,003,988; December in 1991 was announced on the 17th authorizes the people's such as Holeva US5,073,604; With the US5 that authorizes the people such as Liang that announced on February 16th, 1999, in 872,161.
Method for the preparation of the Denture adhesive composition of the present invention that randomly comprises non-binding agent self-supporting layer comprises that the adhesive component with weighed amount is applied on non-binding agent self-supporting layer.The method is disclosed in the US5 that authorizes the people such as Liang that announced on March 2nd, 1999,877,233; The US5 that authorizes the people such as Liang that announced on February 16th, 1999,872,160; The US5 that authorizes the people such as Rajaiah that announced on October 25th, 1996 is in 880,172.
As used in " preparation method of composition " part, use " mixture " to refer to solution, serosity or suspension.
Described adhesive component can adopt several different methods to be coated on non-binding agent self-supporting layer.These comprise: (a) with water-wet non-binding agent self-supporting layer, one or more adhesive component powder are sprinkling upon on wetting layer equably, then the water described layer of moistening again; (b) in one or more adhesive components are water-soluble and/or other one or more solvents, and the gained mixture is coated on described layer; (c) apply described layer with the mixture that makes during the AVE/MA Polymer Processing; (d) when described layer forms, described one or more adhesive components are sneaked in described layer; And (e) in described one or more adhesive components are water-soluble and/or other one or more solvents, on the described layer of gained mixture moistening/be coated on, and the binding agent of one or more powder types is sprinkling upon equably on the layer of moistening/applied, and optionally again applies/described layer of moistening again with described mixture and/or water; (f) with the method for step (e) repeatedly; And (g) above any combination of (a) to (f) middle method.
Disclosed as mentioned, in adhesive component water soluble and/or other solvent, and the gained mixture is coated on described layer.
When making adhesive composition in by one or more adhesive components are water-soluble and/or other solvent, a plurality of embodiments of described method comprise: described polymer is dissolved in one or more solvents of described polymer; Optional binding agent is dissolved in suitable solvent, and the gained mixture is coated on non-binding agent self-supporting layer, then optional one or more binding agents are sprinkling upon on described coat.Can be by the common known technique in this area, comprise extrude, frictioning, spraying, impregnating, realize the coating of layer.
Via a kind of above-mentioned method with polymer deposition after on described layer, then that described layer is dry.Then by Denture adhesive composition is advanced by annular roller or little disintegrating machine or any other suitable device, with its mechanical softening.Then in hydraulic press or flat roller or other suitable device, described compositions is flattened.Then described compositions is die-cut into the artificial tooth shape.These shapes can be conducive to described compositions is administered to artificial tooth.
Following examples have further described with illustration the embodiment in protection domain of the present invention.Given embodiment is only be used to illustrating, can not regarding limitation of the present invention as.In the situation that do not break away from the spirit and scope of the invention, a lot of changes of these embodiment are possible.
Example I
The salt A-J of AVE/MA copolymer
Figure GDA00003036040400181
Figure GDA00003036040400182
Compositions A to J example be used for the salt of the AVE/MA copolymer of Denture adhesive composition of the present invention.
The described component of weighing and when stirring adds in 4 liters of reaction vessels.Use 15% water, with the pre-pulping of all powder except AVE/MA.Then residual powder is washed from chamber wall.Mixture is reacted at the temperature of 80 to 95 ℃.Then with described solution in the baking oven of 65 to 75 ℃ of temperature dry approximately 16 to 24 hours.Then all drying slices are ground to form fine powder.
In addition, as embodiment, can be by making except also having the mixture reaction of the various content NaOH between 0% and 10% ingredients listed above, with above-mentioned salt modification.In addition, as embodiment, the calcium in salt above can be exchanged with magnesium and/or strontium wholly or in part.In addition, as embodiment, the magnesium in salt above can be exchanged with calcium and/or strontium wholly or in part, and strontium is exchanged with magnesium and/or calcium wholly or in part.
Example II
Salt M-O and the R-U of AVE/MA copolymer
Figure GDA00003036040400191
Compositions M-O and R-U example be used for the salt of the AVE/MA copolymer of Denture adhesive composition of the present invention.
The described component of weighing and when stirring adds in 4 liters of reaction vessels.Use 15% water, with the pre-pulping of all powder except AVE/MA.Then residual powder is washed from chamber wall.Mixture is reacted at the temperature of 80 to 95 ℃.Then with described solution in the baking oven of 65 to 75 ℃ of temperature dry approximately 16 to 24 hours.Then all drying slices are ground to form fine powder.
In addition, as embodiment, can be by making except also having the mixture reaction of the various content NaOH between 0% and 10% ingredients listed above, with above-mentioned salt modification.In addition, as embodiment, the calcium in salt above can be exchanged with magnesium and/or strontium wholly or in part.
EXAMPLE III
The salt K-L of AVE/MA copolymer and comparing embodiment P and Q
Figure GDA00003036040400201
Compositions K and L example be used for the salt of the AVE/MA copolymer of Denture adhesive composition of the present invention.Comparing embodiment P and Q example the salt of the AVE/MA copolymer with free acid content outside category of the present invention.
The described component of weighing and when stirring adds in 4 liters of reaction vessels.Use 15% water, with the pre-pulping of all powder except AVE/MA.Then residual powder is washed from chamber wall.Described mixture is heated in being made as the heating jacket of 88.5 ℃, and reaction approximately two hours.Then with described solution in the baking oven of 70 ℃ of temperature dry approximately 22.5 hours.Then all drying slices are ground to form fine powder.
EXAMPLE IV
The evaluation of Denture adhesive composition A1 and A2 and comparative composition C1 and C2
Table 4: Denture adhesive composition
Figure GDA00003036040400211
Table 4A: artificial saliva's compositions
Figure GDA00003036040400212
By compositions listed in table 4, use embodiment salt K, L, P and Q (list in above EXAMPLE III in) make each five (5) grams according to Denture adhesive composition A1 of the present invention and A2 and comparison Denture adhesive composition C1 and C2, then evaluated by specialty grading person.
Described Denture adhesive composition forms according to following method:
By grind the dried AVE/MA salt of disc type thin slice in the Fritsch with 0.08mm screen cloth grinds, at first form the admixture of powder compositions.The compositions of then gained being ground was placed in the 75 ℃ of vacuum drying ovens of 30 inches Hg vacuum that stretched approximately 2 hours.Follow weighing AV/ME salt and mix with CMC in vial.Use vortex agitator that powder was rocked blend approximately 30 seconds.
Then form the hydrated sample compositions: at first with the weighing of 0.5g powder blend to 14mL plasticity polypropylene round bottom tubular type bottle (17 * 100mm type).Then described bottle is placed on VWR Analog vortex agitator, and is set on the #10 shelves.Described bottle is placed on agitator, makes powder curl up in bottle inside with the vortex form.Then via the 10mL syringe, artificial saliva's compositions that 3.0mL is found in table 4A adds (reinforced cost approximately a second) in the vortex that is formed by powder in pipe.When the powder hydration, then continue to mix 3-5 second.Stop agitator, and manually use immediately metallic spatula further to stir gained combination, until the block particle size of gel is down to less than 1mm, and form uniform gel.Top cover is fixed to the bottle top, and wraps up top cover-bottle driving fit line with Parafilm.Then make sample in bottle about 23 ℃ of lower balances approximately 18 hours.
Then by specialty grading person, adopt following method that compositions is relative to each other graded, and result is come together in table 4B.
Use metallic spatula to take out hydrated sample from bottle.Sample is manually stretched and slowly pulls open until breakaway poing.With the broken pieces back pressure together.To each sample, will stretch/rupture/the back pressure step repeats 4-8 time, to evaluate following properties:
Caking property: mainly make sample breakage evaluation by the much power of needs.
Cohesiveness: by sample, the viscosity of finger is evaluated.
Elasticity: by stretching at sample and discharging or resilience degree evaluation during fracture
Healing property again: the uniformity and the difficulty that are again formed the monolithic similar to former by sample are commented
Decide, there is no the phase of seam, agglomerate or separation.
Mealiness: evaluated by caking degree and unevenness that sample after step I v produces.In many feelings
Under condition, this is also with the agglomerate of part drying " look ".
Known provide good retentivity and for the acceptable Denture adhesive of consumer have in-to caking property, cohesiveness and the elasticity (more high better) of-Gao and in-to-low mealiness (more low better).
Table 4B: result
Figure GDA00003036040400231
By the table 4B in as seen, compare with C2 with comparing embodiment C1, provide caking property, cohesiveness, elasticity and mealiness value preferably according to compositions A1 of the present invention and A2.
EXAMPLE V
Can be by following ingredients being blended together to make the Denture adhesive composition that is the cream form:
Figure GDA00003036040400232
Weighing orchil, vaseline and mineral oil, and heating and mixing in glass jar under 50 to 60 ℃ are until visually even.Then weighing powder (colloidal silica, CMC, AVE/MA copolymer salt), and rock-be blended together in container.Afterwards, with scraper, powder is sneaked in liquid, until acquisition is visually uniform pink cream.The experimenter is placed on described cream compositions on artificial tooth.Then the experimenter embeds artificial tooth in his/her mouth, and its pressurization is fixing.Such composition will provide good retentivity and the mouthfeel of improvement.
Example VI
Can be by following ingredients being blended together to make the Denture adhesive composition of powder type:
All components is blended together.Also can be by using the mixture of various AVE/MA salt, with above-mentioned powder composition modification.The experimenter is placed on described compositions on the artificial tooth of pre-moistening, allows its of short duration hydration.Then the experimenter embeds artificial tooth in his/her mouth, and its pressurization is fixing.
Example VII A
Can followingly make the denture stability compositions of wafer form: the non-woven polyester (non-binding agent self-supporting layer) of " taking advantage of 20 " with water-wet 58.Apply equably this humidity strip with following compositions.The water described layer of moistening again afterwards.Described layer is dry.By the described compositions of annular roller mechanical softening, then on hydraulic press, described compositions is flattened.Described compositions is die-cut into desired shape.Moistening, and these wafer set compounds are administered to artificial tooth.Then artificial tooth is embedded in mouth, and its pressurization is fixing.
Figure GDA00003036040400242
EXAMPLE V VII
Can resulting composition be extruded into sheet material by following ingredients is blended together, and be die-cut into desired shape, make the Denture adhesive composition of goods or joint strip form.
Figure GDA00003036040400243
Also can be by using the mixture of various AVE/MA salt, with the above-mentioned composition modification.The experimenter is placed on described compositions on artificial tooth.Then the experimenter embeds artificial tooth in his/her mouth, and its pressurization is fixing.
Example I X
The Denture adhesive cream
Figure GDA00003036040400251
The step of Preparation Example 9A-9B compositions: at first will have wall scraper blade (Unimix derives from Haagen and Rinau) and hot water jacket's agitator and be connected to water-bath and vacuum pump.Hot water jacket's water-bath is made as approximately 95 ℃.Mineral oil, vaseline (if present) and/or microwax are added in stirred vessel.Turn on agitator is 60RPM extremely approximately; Stir until their temperature reaches approximately 95 ℃.Via funnel, AVE/MA salt, carboxymethyl cellulose and silicon dioxide are added in agitator, and open blow vent.Close blow vent and stop stirring.Wipe powder mass off.Restart to stir with the about speed of 60RPM.Apply the approximately vacuum of 24 inches Hg posts, and mixing is until batch of material reaches approximately 90 ℃.To bathe temperature drop to approximately 60 ℃, and continue to stir under vacuum, until batch of material reaches approximately 65 ℃.Stop stirring, close pump, slowly open blow vent and discharge vacuum, and mention capping.Sample is filled in suitable container, is the about metal foil tube of 1.4oz as capacity.
Dimension disclosed herein and value are not intended to be understood to be strictly limited to described exact value.On the contrary, except as otherwise noted, the scope that each such dimension refers to the numerical value quoted and is equal on the function of this numerical value.For example, disclosed dimension " 40mm " is intended to expression " approximately 40mm ".
Except as otherwise noted, all percentage ratios, umber and ratio are all based on the gross weight of the present composition.All based on the content of active substance, therefore except as otherwise noted, they do not comprise solvent or by-product in the material that may be included in commercially available acquisition to all wt of relevant ingredients listed.Herein, term " percentage by weight " can be expressed as " % by weight ".Except as otherwise noted, in the present invention, all molecular weight used are weight average molecular weight.
" comprise/comprise (comprising) " herein, and refer to add other step and other composition that does not affect final result.This term comprises term " by forming " and " basically by forming ".Therefore, the compositions and methods of the invention/process can comprise element of the present invention as herein described and restriction, and any additional or optional member, component, step or restriction as herein described, by element of the present invention as herein described and restriction, and any additional or optional member, component, step or restriction composition as herein described, basically by element of the present invention as herein described and restriction, and any additional or optional member, component, step or restriction as herein described form.
As used herein, term " tooth " refers to nature tooth and artificial teeth or artificial tooth.
All documents of quoting in detailed Description Of The Invention are all incorporated herein by reference in relevant portion; Should not be interpreted as admitting that to quoting of any document it is about prior art of the present invention.When any implication of term in any implication of term in this written document or definition and the file of incorporating into way of reference or when defining contradiction, should obey implication or the definition of giving this term in this written document.
Although illustrated and described specific embodiments of the present invention, it will be apparent to one skilled in the art that in the situation that do not break away from the spirit and scope of the invention and can make a variety of changes and revise.Therefore, claims all these changes and the modification that are intended to be included in the scope of the present invention.

Claims (15)

1. Denture adhesive composition, described compositions comprises:
A) salt of the copolymer of 25% to 45% the alkyl vinyl ether-maleic acid that comprises cationic salts functional group or maleic anhydride by weight of the composition, described cationic salts functional group comprises:
I) 60% to 72% the cation that is selected from calcium, strontium, magnesium or their combination;
Ii) 0% to 10% sodium cation;
Iii) less than 1% zinc cation; With
Iv) 25% to 40% free acid component;
B) by weight of the composition 15% to 25% have 200,000 to 1,000, the carboxymethyl cellulose of 000 daltonian molecular weight; With
C) carrier.
2. Denture adhesive composition as claimed in claim 1, wherein said cationic salts functional group comprises the cation less than 0.0001%, described cation chosen from Fe, manganese, zinc, copper, sodium, potassium, zirconium, strontium, magnesium and/or aluminum.
3. Denture adhesive composition as claimed in claim 1, wherein said cationic salts functional group comprises 25% to 35% described free acid component.
4. Denture adhesive composition as claimed in claim 1, wherein said cationic salts functional group comprises 60% to 72% calcium cation.
5. Denture adhesive composition as claimed in claim 1, wherein said cationic salts functional group is by 60% to 70% calcium cation, and 0% to 5% sodium cation and 25% to 35% described free acid component form.
6. Denture adhesive composition as claimed in claim 1, wherein said cationic salts functional group is by 65% to 70% calcium cation, and 0% to 5% sodium cation and 28% to 32% described free acid component form.
7. the described Denture adhesive composition of claim as aforementioned in any one, wherein said cationic salts functional group comprises the zinc cation less than 0.1%.
8. the described Denture adhesive composition of claim as aforementioned in any one, wherein said carboxymethyl cellulose has 500,000 to 900,000, preferred 600,000 to 800,000 daltonian molecular weight.
9. the described Denture adhesive composition of claim as aforementioned in any one, described compositions also comprise the freely composition of the group of following composition of one or more choosings: additional adhesive component, plasticizer, coloring agent, antiseptic, thickening agent, excipient, flavoring agent, aromatic, sensory agent and their mixture.
10. the described Denture adhesive composition of claim as aforementioned in any one, wherein said adhesive composition is composed of the following components: the salt of the copolymer of alkyl vinyl ether-maleic acid or maleic anhydride, carboxymethyl cellulose and carrier, described carrier comprise water-insoluble liquid, gel, solid thermoplastics or their combination.
11. the described Denture adhesive composition of claim as aforementioned in any one, the salt of the copolymer of wherein said alkyl vinyl ether-maleic acid or maleic anhydride has greater than 1,250,000 molecular weight.
12. the described Denture adhesive composition of claim as aforementioned in any one, wherein when under 25 ℃ in methyl ethyl ketone solution during with the measured in solution of 1%w/v, the salt of the copolymer of alkyl vinyl ether-maleic acid or maleic anhydride has the specific viscosity of 2.5-3.8.
13. the described Denture adhesive composition of claim as aforementioned in any one, wherein said carrier comprises microwax.
14. the described Denture adhesive composition of claim as aforementioned in any one, wherein said compositions comprises the strontium cation less than 0.1%.
15. one kind with Denture adhesive to the method in oral cavity, wherein will the described compositions of claim as aforementioned in any one be administered to artificial tooth, oral cavity or both and the ridge or the palate that afterwards described artificial tooth are fixed to described oral cavity.
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